Granular solid with monodisperse particle size distribution

ABSTRACT

A granular solid with monodisperse particle size distribution is disclosed, which may be obtained by melting an essentially anhydrous composition, which is solid at room temperature and made from at least one cosmetic ingredient. A flow of the melt is dispersed into droplets by means of a casting plate and vibration and said droplets contacted with a cooling medium, which causes the solidification thereof.

FIELD OF THE INVENTION

[0001] The invention is in the field of cosmetics and relates to readilysoluble solids with a monodisperse particle size distribution, to aprocess for their preparation, and to their use for the preparation ofsurface-active preparations, specifically compositions for haircare andbodycare.

PRIOR ART

[0002] The formulation of cosmetic feed materials which are solid atroom temperature, such as, for example, emulsifiers, wax bodies orbodying agents, is usually carried out by spray crystallization.Usually, a number of material pressure nozzles, so-called solid-conenozzles, are installed in the top of the spray towers, via which thefeed materials are atomized into the spray tower. In this process, thestream exiting from the nozzle with high turbulence ruptures after justa short distance from the mouth of the nozzle and forms droplets, therupturing being additionally intensified by the rotation of the stream.The crystallization product prepared in this way has a broad particlesize spectrum. Because of the size content which is produced during thisoperation and the risk of a dust explosion, spraying plants of this typeare subject to increased obligations regarding procedures in case ofaccident, which includes not inconsiderable requirements for operationalsafety and leads to increased costs for the preparation process. Afurther problem consists in the tendency of the spray crystals to caketogether, which considerably increases the expenditure duringincorporation into the end formulations.

[0003] Amongst the producers of cosmetic raw materials, there istherefore lively interest in solids with a narrowed particle sizespectrum, in particular with a negligible fines or dust content (<0.5mm) of less than 1% by weight. At the same time, the desire is forproducts which dissolve more rapidly in an oily or aqueous phase andthus can be incorporated more easily.

[0004] The object of the present invention was therefore to providenovel granular solids which are free from the described disadvantages,i.e. have a monodisperse particle size distribution, virtually no dustcontent and an improved dissolution rate both in an aqueous and an oilymedium.

DESCRIPTION OF THE INVENTION

[0005] The invention provides granular solids with a monodisperseparticle size distribution which are obtainable by liquefying apredominantly anhydrous preparation which is solid at room temperatureand which comprises at least one cosmetic feed material, making a streamof the melt into droplets using a casting plate by vibration, andpassing a cooling medium countercurrently to the droplets, which causesthem to solidify.

[0006] Surprisingly, it has been found that the aim set can be achievedby means of droplet generation which is different from conventionalspray crystallization. Here, the feed mixtures are introduced as meltinto the drop-formation tower via a perforated plate or a die plate. Asa result of an excited membrane, a frequency is impressed onto theliquid, the liquid thread is interrupted again and again and, due to theinterfacial tension, small spheres form which then pass into the actualspraying tower and then, as they fall freely through, for example, acountercurrent stream of dehydrated cold air, are crystallized.Depending on the perforation diameter and membrane oscillationfrequency, it is possible to set a defined particle spectrum withoutdust fraction. A plant of this type is thus no longer subject to theincreased obligations regarding procedures in case of accident, whichleads to a drastic reduction in the technical expenditure and the costsassociated therewith. In addition, in the production of the granulesthere is usually a broad solidification range. The products frequentlyhave one phase in the form of supercooled liquids, meaning thatpost-crystallization is associated with a heat of reaction. This canprevent block formation by the particles sticking together. Finally, anessential advantage consists in the fact that the “beads” obtained inthis way have a significantly improved solubility, compared withconventional supply forms, for example pellets or flakes, both in oilyand aqueous media. Moreover, this substantiates the claim that thesubstances are novel.

[0007] The invention further relates to a process for the preparation ofgranular solids with a monodisperse particle size distribution, in whicha predominantly anhydrous preparation which is solid at room temperatureand which comprises at least one cosmetic feed material is liquefied, astream of the melt is made into droplets using a casting plate byvibration and a cooling medium is passed countercurrently to thedroplets, which causes them to solidify.

[0008] Cosmetic ingredients

[0009] The choice of cosmetic ingredients is unimportant in itselfprovided they are in the form of solids in anhydrous form attemperatures below 25° C., preferably at 18 to 22° C. Suitableingredients are preferably emulsifiers, wax bodies and bodying agents,and mixtures thereof. These are usually used as anhydrous preparations,melted and then formed into drops. It is, however, also possible to usepreparations which are predominantly anhydrous, i.e. in which the waterfraction is less than 50% by weight, preferably less than 25% by weightand in particular less than 5% by weight. This is the case, for example,when anionic or nonionic emulsifiers are used which are often in theform of aqueous surfactant pastes as a result of the preparation.

[0010] Emulsifiers

[0011] Suitable emulsifiers are, for example, nonionogenic surfactantsfrom at least one of the following groups:

[0012] alkyl and/or alkenyl oligoglycosides, fatty acidN-alkylpolyhydroxyalkylamides;

[0013] addition products of from 2 to 30 mol of ethylene oxide and/or 0to 5 mol of propylene oxide onto linear fatty alcohols having 8 to 22carbon atoms, onto fatty acids having 12 to 22 carbon atoms, ontoalkylphenols having 8 to 15 carbon atoms in the alkyl group, andalkylamines having 8 to 22 carbon atoms in the alkyl radical;

[0014] addition products of from 1 to 15 mol of ethylene oxide ontocastor oil and/or hydrogenated castor oil;

[0015] addition products of from 15 to 60 mol of ethylene oxide ontocastor oil and/or hydrogenated castor oil;

[0016] mixed ethers and ethoxylated fatty acid alkyl esters;

[0017] partial esters of glycerol and/or sorbitan with unsaturated,linear or saturated, branched fatty acids having 12 to 22 carbon atomsand/or hydroxycarboxylic acids having 3 to 18 carbon atoms, and adductsthereof having 1 to 30 mol of ethylene oxide;

[0018] partial esters of polyethylene glycol (molecular weight 400 to 5000), trimethylolpropane, pentaerythritol, sugar alcohols (e.g.sorbitol), alkyl glucosides (e.g. methyl glucoside, butyl glucoside,lauryl glucoside), and polyglucosides (e.g. cellulose) with saturatedand/or unsaturated, linear or branched fatty acids having 12 to 22carbon atoms and/or hydroxycarboxylic acids having 3 to 18 carbon atoms,and adducts thereof having 1 to 30 mol of ethylene oxide;

[0019] mixed esters of pentaerythritol, fatty acids, citric acid andfatty alcohol according to German Patent 1165574 and/or mixed esters offatty acids having 6 to 22 carbon atoms, methyl glucose and polyols,preferably glycerol or polyglycerol,

[0020] mono-, di- and trialkyl phosphates, and mono-, di-and/or tri-PEGalkyl phosphates and salts thereof;

[0021] wool wax alcohols;

[0022] polysiloxane-polyalkyl-polyether copolymers or correspondingderivatives;

[0023] block copolymers, e.g. polyethylene glycol-30dipolyhydroxystearates;

[0024] polymer emulsifiers, e.g. Pemulen grades (TR-1, TR-2) fromGoodrich;

[0025] polyalkylene glycols and

[0026] glycerol carbonate.

[0027] Alkyl and alkenyl oligoglycosides are known nonionic surfactantswhich conform to the formula (I)

R¹O—[G]_(p)  (I)

[0028] in which R¹ is an alkyl and/or alkenyl radical having 4 to 22carbon atoms, G is a sugar radical having 5 or 6 carbon atoms and p is anumber from 1 to 10. They can be obtained by appropriate processes ofpreparative organic chemistry. As representative for the extensiveliterature, reference may be made here to the specifications EP-A10301298 and WO 90/03977. The alkyl and/or alkenyl oligoglycosides can bederived from aldoses or ketoses having 5 or 6 carbon atoms, preferablyfrom glucose. The preferred alkyl and/or alkenyl oligoglycosides arethus alkyl and/or alkenyl oligoglucosides. The index number p in thegeneral formula (I) gives the degree of oligomerization (DP), i.e. thedistribution of mono- and oligoglycosides and is a number between 1 and10. While p in a given compound must always be an integer and can hereprimarily assume the values p=1 to 6, the value p for a certain alkyloligoglycoside is an analytically determined calculated parameter whichis in most cases a fraction. Preference is given to using alkyl and/oralkenyl oligoglycosides having an average degree of oligomerization p offrom 1.1 to 3.0. From a performance viewpoint, preference is given tothose alkyl and/or alkenyl oligoglycosides whose degree ofoligomerization is less than 1.7 and is in particular between 1.2 and1.4. The alkyl or alkenyl radical R¹ can be derived from primaryalcohols having 4 to 11, preferably 8 to 10 carbon atoms. Typicalexamples are butanol, caproic alcohol, caprylic alcohol, capric alcoholand undecyl alcohol, and technical-grade mixtures thereof, as areobtained, for example, in the hydrogenation of technical-grade fattyacid methyl esters or in the course of the hydrogenation of aldehydesfrom the Roelen oxo synthesis. Preference is given to alkyloligoglucosides of chain length C₈-C₁₀ (DP=1 to 3) which are produced asforerunnings during the distillative separation of technical-gradeC₈-C₁₈-coconut fatty alcohol and may be contaminated with a content ofless than 6% by weight of C₁₂-alcohol, and also alkyl oligoglucosidesbased on technical-grade C_(9/11)-oxo alcohols (DP=1 to 3). The alkyl oralkenyl radical R¹ can also be derived from primary alcohols having 12to 22, preferably 12 to 14, carbon atoms. Typical examples are laurylalcohol, myristyl alcohol, cetyl alcohol, palmoleyl alcohol, stearylalcohol, isostearyl alcohol, oleyl alcohol, elaidyl alcohol,petroselinyl alcohol, arachyl alcohol, gadoleyl alcohol, behenylalcohol, erucyl alcohol, brassidyl alcohol, and technical-grade mixturesthereof which can be obtained as described above. Preference is given toalkyl oligoglucosides based on linear or branched fatty alcohols having8 8 to 18 or 16 to 18 or carbon atoms, in particular technical-gradecoconut fatty alcohol or cetearyl alcohol or isostearyl alcohol.

[0029] Fatty acid N-alkylpolyhydroxyalkylamides are likewise suitablenonionic emulsifiers which preferably conform to the formula (II)

[0030] in which R²CO is an aliphatic acyl radical having 6 to 22 carbonatoms, R³ is an alkyl or hydroxyalkyl radical having 1 to 4 carbon atomsand [Z] is a linear or branched polyhydroxyalkyl radical having 3 to 12carbon atoms and 3 to 10 hydroxyl groups. The fatty acidN-alkylpolyhydroxyalkylamides are known substances which can usually beobtained by a reductive amination of a reducing sugar with an alkylamineor an alkanolamine and subsequent acylation with a fatty acid, a fattyacid alkyl ester or a fatty acid chloride. With regard to processes fortheir preparation, reference is made to the U.S. patent U.S. Pat. No.1,985,424, U.S. Pat. No. 2,016,962 and U.S. Pat. No. 2,703,798, and theinternational patent application WO 92/06984. A review of this topic isgiven by H. Kelkenberg in Tens.Surf. Deterg. 25, 8 (1988). The fattyacid N-alkylpolyhydroxyalkylamides are preferably derived from reducingsugars having 5 or 6 carbon atoms, in particular from glucose. Thepreferred fatty acid N-alkylpolyhydroxyalkylamides are thus fatty acidN-alkylglucamides, as given by the formula (III):

[0031] As fatty acid N-alkylpolyhydroxyalkylamides, preference is givento using glucamides of the formula (III) in which R³ is an alkyl groupand R²CO is the acyl radical of caproic acid, caprylic acid, capricacid, lauric acid, myristic acid, palmitic acid, palmoleic acid, stearicacid, isostearic acid, oleic acid, elaidic acid, petroselic acid,linoleic acid, linolenic acid, arachidic acid, gadoleic acid, behenicacid or erucic acid or technical-grade mixtures thereof. Particularpreference is given to fatty acid N-alkylglucamides of the formula (III)which are obtained by reductive animation of glucose with methylamineand subsequent acylation of palmitic, stearic and/or isostearic acid ora corresponding derivative. In addition, the polyhydroxyalkylamides canalso be derived from maltose and palatinose.

[0032] The addition products of ethylene oxide and/or of propylene oxideonto fatty alcohols, fatty acids, alkylphenols or onto castor oil areknown, commercially available products. These are homolog mixtures whoseaverage degree of alkoxylation corresponds to the ratio of thequantitative amounts of ethylene oxide and/or propylene oxide andsubstrate with which the addition reaction is carried out. These arepreferably addition products of from 5 to 50 and in particular 10 to 20mol of ethylene oxide onto fatty alcohols having 12 to 22 and preferably16 to 18 carbon atoms.

[0033] Typical examples of suitable ethoxylated partial glycerides areaddition products of from 1 to 30, preferably 5 to 10, mol of ethyleneoxide onto hydroxystearic acid monoglyceride, hydroxystearic aciddiglyceride, isostearic acid monoglyceride, isostearic acid diglyceride,oleic acid monoglyceride, ricinoleic acid moglyceride, ricinoleic aciddiglyceride, linoleic acid monoglyceride, linoleic acid diglyceride,linolenic acid monoglyceride, linolenic acid diglyceride, erucic acidmonoglyceide, erucic acid diglyceride, tartaric acid monoglyceride,tartaric acid diglyceride, citric acid monoglyceride, citric [lacuna]diglyceride, malic acid monoglyceride, malic acid diglyceride, andtechnical-grade mixtures thereof, which may also comprise to a minordegree small amounts of triglyceride from the preparation process.[lacuna] sorbitan esters are sorbitan monoisostearate, sorbitansesquiisostearate, sorbitan diisostearate, sorbitan triisostearate,sorbitan monooleate, sorbitan sesquioleate, sorbitan dioleate, sorbitantrioleate, sorbitan monoerucate, sorbitan sesquierucate, sorbitandierucate, sorbitan trierucate, sorbitan monoricinoleate, sorbitansesquiricinoleate, sorbitan diricinoleate, sorbitan triricinoleate,sorbitan monohydroxystearate, sorbitan sesquihydroxystearate, sorbitandihydroxystearate, sorbitan trihydroxystearate, sorbitan monotartrate,sorbitan sesquitartrate, sorbitan ditartrate, sorbitan tritartrate,sorbitan monocitrate, sorbitan sesquicitrate, sorbitan dicitrate,sorbitan tricitrate, sorbitan monomaleate, sorbitan sesquimaleate,sorbitan dimaleate, sorbitan trimaleate, and technical-grade mixturesthereof. Also suitable are addition products of from 1 to 30, preferably5 to 10, mol of ethylene oxide onto said sorbitan esters.

[0034] Typical examples of suitable polyglycerol esters are the polyolpoly-12-hydroxystearates. These are known substances which aredescribed, for example, in the international patent application WO95/34528 (Henkel). The polyol component of the emulsifiers can bederived from substances which have at least two, preferably 3 to 12 andin particular 3 to 8, hydroxyl groups and 2 to 12 carbon atoms. Typicalexamples are:

[0035] (a) glycerol and polyglycerol;

[0036] (b) alkylene glycols, such as, for example, ethylene glycol,diethylene glycol, propylene glycol;

[0037] (c) methyol compounds, such as, in particular, trimethylolethane,trimethylolpropane, tri-methylolbutane, pentaerythritol anddipenta-erythritol;

[0038] (d) alkyl oligoglucosides having 1 to 22, preferably 1 to 8 andin particular 1 to 4, carbon atoms in the alkyl radical, such as, forexample, methyl glucoside and butyl glucoside;

[0039] (e) sugar alcohols having 5 to 12 carbon atoms, such as, forexample, sorbitol or mannitol,

[0040] (f) sugars having 5 to 12 carbon atoms, such as, for example,glucose or sucrose;

[0041] (g) amino sugars, such as, for example, glucamine. Among theemulsifiers to be used according to the invention, reaction productsbased on polyglycerol are of particular importance due to theirexcellent performance properties. It has proven particularlyadvantageous to use selected polyglycerols which have the followinghomolog distribution (the preferred ranges are given in brackets):Glycerol  5 to 35 (15 to 30) % by weight Diglycerols 15 to 40 (20 to 32)% by weight Triglycerols 10 to 35 (15 to 25) % by weight Tetraglycerols 5 to 20 (8 to 15) % by weight Pentaglycerols  2 to 10 (3 to 8) % byweight Oligoglycerols ad 100 % by weight

[0042] Further suitable polyglycerol esters arepolyglycerol-3-diisostearate (Lameform® TGI), polyglyceryl-4 isostearate(Isolan® GI 34), polyglyceryl-3 oleate, diisostearoyl polyglyceryl-3diisostearate (Isolan® PDI), polyglyceryl-3 methylglucose distearate(Tego Care® 450), polyglyceryl-3 beeswax (Cera Bellina®), polyglyceryl-4caprate (polyglycerol caprate T2010/90), polyglyceryl-3 cetyl ether(Chimexane® NL), polyglyceryl-3 distearate (Cremophor® GS 32) andpolyglyceryl polyricinoleate (Admul® WOL 1403) polyglyceryl dimerateisostearate, and mixtures thereof. Examples of further suitable polyolesters are the mono-, di- and triesters of trimethylolpropane orpentaerythritol with lauric acid, coconut fatty acid, tallow fatty acid,palmitic acid, stearic acid, oleic acid, behenic acid and the like,which have optionally been reacted with 1 to 30 mol of ethylene oxide.

[0043] Suitable nonionic emulsifiers are, in particular, also mixedethers or hydroxy mixed ethers, which are reaction products of the fattyalcohol polyglycol ethers already given with C₁-C₈ alkyl halides orC₈-C₁₂ epoxides. Also suitable are alkoxylated fatty acid lower alkylesters which are obtained by, for example, inserting 1 to 10 mol ofethylene oxide into the ester bond of C₁₂-C₁₈-fatty acid methyl esters.This is possible, inter alia, by reacting the esters with ethylene oxidein the presence of calcined hydrotalcites as catalysts.

[0044] It is also possible to use zwitterionic surfactants asemulsifiers. The term “zwitterionic surfactants” is used to refer tothose surface-active compounds which carry, in the molecule, at leastone quaternary ammonium group and at least one carboxylate group and onesulfonate group. Particularly suitable zwitterionic surfactants are theso-called betaines, such as the N-alkyl-N,N-dimethylammonium glycinates,for example cocoalkyldimethylammonium glycinate,N-acylaminopropyl-N,N-dimethylammonium glycinates, for examplecocoacylaminopropyldimethylammonium glycinate, and2-alkyl-3-carboxymethyl-3-hydroxyethylimidazolines each having 8 to 18carbon atoms in the alkyl or acyl group, and cocoacylaminoethylhydroxyethylcarboxymethyl glycinate. Particular preference is given tothe fatty acid amide derivative known under the CTFA name CocamidopropylBetaine. Likewise suitable emulsifiers are ampholytic surfactants.Ampholytic surfactants are to be understood as meaning thosesurface-active compounds which, apart from containing a C_(8/18)-alkylor-acyl group in the molecule, contain at least one free amino group andat least one—COOH or—SO₃H group and are capable of forming internalsalts. Examples of suitable ampholytic surfactants are N-alkylglycines,N-alkylpropionic acids, N-alkylaminobutyric acids,N-alkyliminodipropionic acids,N-hydroxyethyl-N-alkylamidopropylglycines, N-alkyltaurines,N-alkylsarcosines, 2-alkylaminopropionic acids and alkylaminoaceticacids each having about 8 to 18 carbon atoms in the alkyl group.Particularly preferred ampholytic surfactants areN-cocoalkylaminopropionate, cocoacyl-aminoethylaminopropionate andC_(12/18) acylsarcosine. Finally, cationic surfactants are also suitableas emulsifiers, those of the ester quat type, preferablymethyl-quaternized difatty acid triethanolamine ester salts, beingparticularly preferred.

[0045] Wax Bodies

[0046] Typical examples of suitable wax bodies which can be made intodrops for the purposes of the invention are, for example, natural waxes,such as, for example, candelilla wax, carnauba wax, Japan wax, espartograss wax, cork wax, guaruma wax, rice germ oil wax, sugarcane wax,ouricury wax, montan wax, beeswax, shellac wax, spermaceti, lanolin(wool wax), uropygial grease, ceresine, ozokerite (earth wax),petrolatum, paraffin waxes, microcrystalline waxes; chemically modifiedwaxes (hard waxes), such as, for example, montan ester waxes, sasolwaxes, hydrogenated jojoba waxes, and synthetic waxes, such as, forexample esters of fatty acids with fatty alcohols, polyalkylene waxesand polyethylene glycol waxes in question.

[0047] In addition to the fats, suitable additives are also fat-likesubstances, such as lecithins and phospholipids. The term lecithins isunderstood by the person skilled in the art as meaning thoseglycerophospholipids which form from fatty acids, glycerol, phosphoricacid and choline by esterification. In the specialist field, lecithinsare therefore also often referred to as phosphatidylcholines (PC).Examples of natural lecithins which may be mentioned are cephalins,which are also referred to as phosphatidic acids and are derivatives of1,2-diacyl-sn-glycerol-3-phosphoric acids. By contrast, the term“phospholipids” usually means mono- and, preferably, diesters ofphosphoric acid with glycerol (glycerol phosphates) which are generallyconsidered to be fats. In addition, sphingosines and sphingolipids arealso suitable.

[0048] Examples of suitable pearlescent waxes are: alkylene glycolesters, specifically ethylene glycol distearate; fatty acidalkanolamides, specifically coconut fatty acid diethanolamide; partialglycerides, specifically stearic acid monoglyceride; esters ofpolyhydric, optionally hydroxy-substituted, carboxylic acids with fattyalcohols having 6 to 22 carbon atoms, specifically long-chain esters oftartaric acid; fatty substances, such as, for example, fatty ketones,fatty aldehydes, fatty ethers and fatty carbonates which have, in total,at least 24 carbon atoms, specifically laurone and distearyl ether;fatty acids, such as stearic acid, hydroxystearic acid or behenic acid,ring-opening products of olefin epoxides having 12 to 22 carbon atomswith fatty alcohols having 12 to 22 carbon atoms and/or polyols having 2to 15 carbon atoms and 2 to 10 hydroxyl groups, and mixtures thereof.

[0049] Bodying Agents

[0050] The most important group of bodying agents which can be formedinto drops are the fatty alcohols. These are to be understood as meaningprimary aliphatic alcohols which preferably conform to the formula (IV)

R⁴OH   (IV)

[0051] in which R⁴ is an aliphatic, linear or branched hydrocarbonradical having 6 to 22 carbon atoms and 0 and/or 1, 2 or 3 double bonds.Typical examples are caproic alcohol, caprylic alcohol, 2-ethylhexylalcohol, capric alcohol, lauryl alcohol, isotridecyl alcohol, myristylalcohol, cetyl alcohol, palmoleyl alcohol, stearyl alcohol, isostearylalcohol, oleyl alcohol, elaidyl alcohol, petroselinyl alcohol, linoleylalcohol, linolenyl alcohol, eleostearyl alcohol, arachyl alcohol,gadoleyl alcohol, behenyl alcohol, erucyl alcohol and brassidyl alcohol,and technical-grade mixtures thereof which are produced, for example,during the high-pressure hydrogenation of technical-grade methyl estersbased on fats and oils or aldehydes from the Roelen oxosynthesis, and asmonomer fraction in the dimerization of unsaturated fatty alcohols.Preference is given to technical-grade linear and/or branched fattyalcohols having 16 to 18 carbon atoms, such as, for example cetearylalcohol or isostearyl alcohol.

[0052] Further suitable bodying agents are partial glycerides, i.e.monoglycerides, diglycerides and technical-grade mixtures thereof arealso suitable as additives and may, as a result of the preparation, alsocomprise small amounts of triglycerides. The partial glyceridespreferably conform to the formula (V)

[0053] in which R⁵CO is a linear or branched, saturated and/orunsaturated acyl radical having 6 to 22, preferably 12 to 18, carbonatoms, R⁶ and R⁷, independently of one another, are R⁵CO or OH and thesum (m+n+p) is 0 or numbers from 1 to 100, preferably 5 to 25, with theproviso that at least one of the two radicals R⁶ and R⁷ is OH. Typicalexamples are mono- and/or diglycerides based on caproic acid, caprylicacid, 2-ethylhexanoic acid, capric acid, lauric acid, isotridecanoicacid, myristic acid, palmitic acid, palmoleic acid, stearic acid,isostearic acid, oleic acid, elaidic acid, petroselic acid, linoleicacid, linolenic acid, eleostearic acid, arachidic acid, gadoleic acid,behenic acid and erucic acid, and technical-grade mixtures thereof.Preference is given to using technical-grade cetearyl glycerides,palmitic acid glycerides, stearic acid glycerides and/or isostearic acidglycerides which have a monoglyceride content in the range from 50 to95% by weight, preferably 60 to 90% by weight.

[0054] Special Mixtures

[0055] In a preferred embodiment of the present invention, sugarsurfactants of the alkyl oligoglucoside type are used together withbodying agents from the group of fatty alcohols where it is advisable touse representatives which have identical alkyl radicals since these notonly have performance advantages, but are also of interest economicallysince they are already produced as intermediates during the synthesis ofthe glucosides. Drops are very particularly preferably made from thosemixtures which comprise alkyl oligoglucosides of the formula (I) andfatty alcohols of the formula (IV) in which R¹ and R⁴ are linear orbranched alkyl radicals having 16 to 18 carbon atoms, specificallycetearyl or isostearyl radicals in the weight ratio 10:90 to 90:10 andspecifically 40:60 to 60:40. The glucoside/fatty alcohol ratio can beadjusted, for example, through the choice of fatty alcohol excess in theacetalation. Subsequently, fatty alcohol can be removed by, for example,extraction in the near-critical range or molecular distillation. Suchproducts, even when in nongranular form, are available commercially, forexample under the names Emulgade® PL 68/50 or Montanov® 68.

[0056] In a further preferred embodiment, drops are made from mixtureswhich comprise alkyl oligoglucosides of the formula (I) in which R¹[lacuna] a linear or branched alkyl radical having 8 to 18 carbon atoms,and polyglycerol poly-12-hydroxystearates in the weight ratio 40:60 to60:40 and in particular 50:50. Such products, even when in nongranularform, are available commercially under the name Eumulgin® VL 75.

[0057] Drop Formation

[0058] The drop formation carried out for the purposes of the process ofthe invention using a vibrating casting plate with excited membrane isalready known for the processing of resins and low-viscosity polyesters.Appropriate components are sold, for example, by Rieter-Automatik underthe name “Droppo Line” for use in textile technology. For the purposesof the process of the invention, preference is given to those castingplates which consist of a heatable upper and lower plate. The lowerplate is usually in the form of a perforated disk, through whoseopenings or channels or capillary nozzles or dropping tubes the dropsthen pass into the spraying tower. In a particular embodiment of theprocess, the nozzles are designed so that, as well as the startingmaterial stream, they also permit the feed of an additional stream ofgas (“control air”), with which the droplets can be further nebulized.This stream of gas can be preheated, for example to 100 to 120° C.,meaning that any traces of water still present in the starting materialare evaporated with its help. The capacity of perforated disks whichusually have 10 to 750 bores may preferably be in the range from 0.3 to3 kg/h/bore, the diameter of the bores is between 0.25 and 1.4 mm. Here,granules are obtained which have a diameter of from 1.6 to 2.7 times thediameter of the bores.

[0059] The oscillation frequency of the perforated plates (“droppingplates”) is typically in the range from 100 to 10 000 and preferably 200to 800 Hz. It can be generated via an excited membrane, an oscillatingplunger, a vibrating plate or sonic excitation.

[0060] A further advantage over conventional processes is also that itis possible to work at a pressure which is only slightly aboveatmospheric pressure (typically: 100 to 4 000 mbar). The temperaturewith which the feed materials are conveyed into the dropping tower islimited by the solidification range and is usually in the range from 40to 100° C., where it must be ensured that the starting materials are notoverheated since this may lead to decomposition and caking. Feedtemperatures which are 3 to 10° C. above the solidification point of thefeed materials have proven particularly effective. The startingmaterials usually have a viscosity of less than 500 mPas (Brookfield,spindle 1, 20° C., 10 rpm). The drops fall downward perpendicularly inareas of low turbulence in the tower. The probability of two or moredrops meeting and caking together to form a so-called “raspberrygranule” is low. Although in principle cooling can take place with acold liquid, for practical reasons cooling in the dropping tower usingcold air in countercurrent is advisable, as is adequately described inthe prior art. The granules are almost spherical and, depending on theorifices in the perforated plate and the frequency, have averagediameters in the range from 1 to 2.5 mm. If desired, the spraying towercan be equipped with a shaking-screen floor in order to make theparticle size distribution even more homogeneous.

[0061] The dust fraction, e.g. particles with particle sizes of lessthan 0.3 mm is virtually zero in this process, and therefore noapparatuses are required to separate off the dust from the exit air. Inthe absence of dust, a circulatory gas procedure is possible, whichleads to a reduction in dehumidification expenditure for introducedfresh air. Instead of air, because of the circulatory gas procedure, itis of course also possible to use inert gas.

[0062] For products with residual heat and with aftercrystallizationheat, an aftercooling section may be connected downstream of thedropping tower. Examples of suitable aftercoolers are gas-permeatedfluidized, fixed or sliding beds, liquid-cooled helical conveyors,pneumatic conveyors or aftercooling belts. For products which firstlyform a supercooled liquid prior to solidification, the crystallizationmay be stimulated by adding inert nucleating agents to the melt or intothe gaseous stream, forcing a secondary stream into the nozzle(rotational flow), dropping the drops through a sonar field, e.g.low-frequency or an ultrasound field or the known generation ofsatellite drops by changing the frequency.

[0063] Industrial Applicability

[0064] The invention further provides for the use of the granular solidsfor preparing surface-active, primarily cosmetic, preparations, inparticular for the field of skincare and haircare compositions. Theycan, however, also be used for the field of oral and dental hygiene, andfor laundry detergents, dishwashing detergents, cleaners and handmodifiers. The use amount of the granules is in the range from 1 to 70%by weight, preferably 5 to 50% by weight and in particular 15 to 35% byweight, based on the compositions.

[0065] These compositions can also comprise, as further auxiliaries andadditives, mild surfactants, oily bodies, thickeners, superfattingagents, stabilizers, polymers, silicone compounds, fats, waxes,lecithins, phospholipids, biogenic active ingredients, UV lightprotection factors, antioxidants, deodorants, antiperspirants,antidandruff agents, film formers, swelling agents, insect repellents,self-tanning agents, tyrosine inhibitors (depigmentation agents),hydrotropes, solubilizers, preservatives, perfume oils, dyes and thelike. In a particular embodiment of the invention, it is also possiblethat the additives described here and below in more detail can be madeinto drops together with the cosmetic ingredients and then be used as a“compound” mixture. This applies in particular to UV light protectionfilters, antioxidants and biogenic active ingredients, where it is alsoa criterion here again that the additives should as far as possible besolid at room temperature.

[0066] Surfactants Surface-active substances which may be present areanionic, nonionic, cationic and/or amphoteric or amphoteric surfactants,the content of which in the compositions is usually about 1 to 70% byweight, preferably 5 to 50% by weight and in particular 10 to 30% byweight. Typical examples of anionic surfactants are soaps,alkylbenzenesulfonates, alkanesulfonates, olefinsulfonates, alkyl ethersulfonates, glyceryl ether sulfonates, α-methyl ester sulfonates, sulfofatty acids, alkyl sulfates, fatty alcohol ether sulfates, glycerolether sulfates, fatty acid ether sulfates, hydroxy mixed ether sulfates,monoglyceride (ether) sulfates, fatty acid amide (ether) sulfates, mono-and dialkyl sulfosuccinates, mono- and dialkyl sulfosuccinamates,sulfotriglycerides, amide soaps, ether carboxylic acids and saltsthereof, fatty acid isethionates, fatty acid sarcosinates, fatty acidtaurides, N-acylamino acids, such as, for example, acyl lactylates, acyltartrates, acyl glutamates and acyl aspartates, alkyl oligoglucosidesulfates, protein fatty acid condensates (in particular vegetableproducts based on wheat) and alkyl (ether) phosphates. If the anionicsurfactants contain polyglycol ether chains, these may have aconventional homolog distribution, but preferably have a narrowedhomolog distribution. Typical examples of nonionic surfactants are fattyalcohol polyglycol ethers, alkylphenol polyglycol ether, fatty acidpolyglycol esters, fatty acid amide polyglycol ethers, fatty aminepolyglycol ethers, alkoxylated triglycerides, mixed ethers or mixedformals, or glucoronic acid derivatives, protein hydrolyzates (inparticular vegetable products based on wheat), polyol fatty acid esters,sugar esters, sorbitan esters, polysorbates and amine oxides. If thenonionic surfactants contain polyglycol ether chains, these may have aconventional homolog distribution, but preferably have a narrowedhomolog distribution. Typical examples of cationic surfactants arequaternary ammonium compounds, such as, for example,dimethyldistearylammonium chloride and ester quats, in particularquaternized fatty acid trialkanolamine ester salts. Typical examples ofamphoteric or zwitterionic surfactants are alkylbetaines,alkylamidobetaines, aminopropionates, aminoglycinates, imidazoliniumbetaines and sulfobetaines. Said surfactants are all known compounds.With regard to the structure and the preparation of the substances,reference may be made to the relevant review papers, for example J.Falbe (ed.), “Surfactants in Consumer Products” Springer Verlag, Berlin,1987, p. 54-124 or J. Falbe (ed.), “Katalysatoren, Tenside undMineralöladditive”, Thieme Verlag, Stuttgart, 1978, p. 123-217. Typicalexamples of particularly suitable mild, i.e. particularlyskin-compatible, surfactants are fatty alcohol polyglycol ethersulfates, monoglyceride sulfates, mono- and/or dialkyl sulfosuccinates,fatty acid isethionates, fatty acid sarcosinates, fatty acid taurides,fatty acid glutamates, α-olefinsulfonates, ether carboxylic acids, alkyloligoglucosides, fatty acid glucamides, alkylamidobetaines, amphoacetalsand/or protein fatty acid condensates, these last preferably being basedon wheat proteins.

[0067] Oily Bodies [lacuna] oily bodies are, for example, Guerbetalcohols based on fatty alcohols having 6 to 18, preferably 8 to 10,carbon atoms, esters of linear C₆-C₂₂-fatty acids with linearC₆-C₂₂-fatty alcohols, esters of branched C₆-C₁₃-carboxylic acids withlinear C₆-C₂₂-fatty alcohols, such as, for example, myristyl myristate,myristyl palmitate, myristyl stearate, myristyl isostearate, myristyloleate, myristyl behenate, myristyl erucate, cetyl myristate, cetylpalmitate, cetyl stearate, cetyl isostearate, cetyl oleate, cetylbehenate, cetyl erucate, stearyl myristate, stearyl palmitate, stearylstearate, stearyl isostearate, stearyl oleate, stearyl behenate, stearylerucate, isostearyl myristate, isostearyl palmitate, isostearylstearate, isostearyl isostearate, isostearyl oleate, isostearylbehenate, isostearyl oleate, oleyl myristate, oleyl palmitate, oleylstearate, oleyl isostearate, oleyl oleate, oleyl behenate, oleylerucate, behenyl myristate, behenyl palmitate, behenyl stearate, behenylisostearate, behenyl oleate, behenyl behenate, behenyl erucate, erucylmyristate, erucyl palmitate, erucyl stearate, erucyl isostearate, erucyloleate, erucyl behenate and erucyl erucate. Also suitable are esters oflinear C₆-C₂₂-fatty acids with branched alcohols, in particular2-ethylhexanol, esters of C₁₈-C₃₈-alkylhydroxy carboxylic acids withlinear or branched C₆-C₂₂-fatty alcohols (cf. DE 19756377 A1), inparticular dioctyl malate, esters of linear and/or branched fatty acidswith polyhydric alcohols (such as e.g. propylene glycol, dimerdiol ortrimertriol) and/or Guerbet alcohols, triglycerides based onC₆-C₁₀-fatty acids, liquid mono-/di-/triglyceride mixtures based onC₆-C₁₈-fatty acids, esters of C₆-C₂₂-fatty alcohols and/or Guerbetalcohols with aromatic carboxylic acids, in particular benzoic acid,esters of C₂-C₁₂-dicarboxylic acids with linear or branched alcoholshaving 1 to 22 carbon atoms or polyols having 2 to 10 carbon atoms and 2to 6 hydroxyl groups, vegetable oils, branched primary alcohols,substituted cyclohexanes, linear and branched C₆-C₂₂-fatty alcoholcarbonates, such as, for example, dicaprylyl carbonate, Guerbetcarbonates, esters of benzoic acid with linear and/or branchedC₆-C₂₂-alcohols (e.g. Finsolv® TN), linear or branched, symmetrical orasymmetrical dialkyl ethers having 6 to 22 carbon atoms per alkyl group,such as, for example, dicaprylyl ether, ring-opening products ofepoxidized fatty acid esters with polyols, silicone oils(cyclomethicone, silicon methicon grades etc.) and/or aliphatic ornaphthenic hydrocarbons, such as, for example, such as squalane,squalene or dialkylcyclohexanes under consideration.

[0068] Thickeners

[0069] Suitable thickeners are hydroxy fatty alcohols having 12 to 22,and preferably 16 to 18, carbon atoms and also fatty acids or hydroxyfatty acids. Suitable thickeners are, for example, Aerosil grades(hydrophilic silicas), polysaccharides, in particular xanthan gum,guar-guar, agar-agar, alginates and Tyloses, carboxymethylcellulose andhydroxyethylcellulose, and also relatively high molecular weightpolyethylene glycol mono- and diesters of fatty acids, polyacrylates,(e.g. Carbopols® and Pemulen grades from Goodrich; Synthalens® fromSigma; Keltrol grades from Kelco; Sepigel grades from Seppic; Salcaregrades from Allied Colloids), polyacrylamides, polymers, polyvinylalcohol and polyvinylpyrrolidone, surfactants, such as, for example,ethoxylated fatty acid glycerides, esters of fatty acids with polyols,such as, for example, pentaerythritol or trimethylolpropane, fattyalcohol ethoxylates with narrowed homolog distribution or alkyloligoglucosides, and electrolytes such as sodium chloride and ammoniumchloride.

[0070] Superfatting Agents

[0071] Superfatting agents which can be used are substances such as, forexample, lanolin and lecithin, and polyethoxylated or acylated lanolinand lecithin derivatives, polyol fatty acid esters, monoglycerides andfatty acid alkanolamides, these last also serving as foam stabilizers.

[0072] Stabilizers

[0073] Stabilizers which can be used are metal salts of fatty acids,such as, for example, the stearates or ricinoleates of magnesium,aluminum and/or zinc.

[0074] Polymers

[0075] Suitable cationic polymers are, for example, cationic cellulosederivatives, such as, for example, a quaternized hydroxyethylcellulosewhich is available under the name Polymer JR 400® from Amerchol,cationic starch, copolymers of diallylammonium salts and acrylamides,quaternized vinylpyrrolidone/vinyl imidazole polymers, such as, forexample, Luviquat® (BASF), condensation products of polyglycols andamines, quaternized collagen polypeptides, such as, for example,lauryldimonium hydroxypropyl hydrolyzed collagen (Lamequat®L/Grünau),quaternized wheat polypeptides, polyethyleneimine, cationic siliconepolymers, such as, for example, amodimethicones, copolymers of adipicacid and dimethylamino hydroxypropyldiethylenetriamine(Cartaretine®/Sandoz), copolymers of acrylic acid withdimethyldiallylammonium chloride (Merquat® 550/Chemviron),polyaminopolyamides, as described, for example, in FR 2252840 A, andcrosslined water-soluble polymers thereof, cationic chitin derivatives,such as, for example, quaternized chitosan, optionally inmicrocrystalline dispersion, condensation products from dihaloalkyls,such as, for example, dibromobutane with bisdialkylamines, such as, forexample, bisdimethylamino-1,3-propane, cationic guar gum, such as, forexample, Jaguar® CBS, Jaguar® C-17, Jaguar® C-16 from Celanese,quaternized ammonium salt polymers, such as, for example, Mirapol® A-15,Mirapol® AD-1, Mirapol® AZ-1 from Miranol.

[0076] Suitable anionic, zwitterionic, amphoteric and nonionic polymersare, for example, vinyl acetate/crotonic acid copolymers,vinylpyrrolidone/vinyl acrylate copolymers, vinyl acetate/butylmaleate/isobornyl acrylate copolymers, methyl vinyl ether/maleicanhydride copolymers and esters thereof, uncrosslinked polyacrylic acidsand polyacrylic acids crosslinked with polyols,acrylamidopropyltrimethylammonium chloride/acrylate copolymers,octylacrylamide/methyl methacrylate/tert-butylaminoethylmethacrylate/2-hydroxypropylmethacrylate copolymers,polyvinylpyrrolidone, vinylpyrrolidone/vinyl acetate copolymers,vinylpyrrolidone/dimethylaminoethyl methacrylate/-vinylcaprolactamterpolymers, and optionally derivatized cellulose ethers and silicones.Further suitable polymers and thickeners are listed in Cosmetics &Toiletries 108, 95 [1993].

[0077] Suitable silicone compounds are, for example,dimethylpolysiloxanes, methylphenylpolysiloxanes, cyclic silicones andamino-, fatty-acid-, alcohol-, polyether-, epoxy-, fluorine-, glycoside-and/or alkyl-modified silicone compounds which can either be liquid orin resin form at room temperature. Also suitable are simethicones, whichare mixtures of dimethicones having an average chain length of from 200to 300 dimethylsiloxane units and hydrogenated silicates. A detailedreview of suitable volatile silicones can additionally be found in Toddet al. in Cosm. Toil. 91, 27 (1976).

[0078] UV Light Protection Filters and Antioxidants

[0079] The term “UV light protection factors” means, for example,organic substances (light protection filters) which are liquid orcrystalline at room temperature and which are able to absorb ultravioletrays and give off the absorbed energy again in the form oflonger-wavelength radiation, e.g. heat. UVB filters can be oil-solubleor water-soluble. Examples of oil-soluble substances are:

[0080] 3-benzylidenecamphor or 3-benzylidenenorcamphor and derivativesthereof, e.g. 3-(4-methylbenzylidene)-camphor, as described in EP0693471 B1;

[0081] 4-aminobenzoic acid derivatives, preferably 2-ethylhexyl4-(dimethylamino)benzoate, 2-octyl 4-(dimethylamino)benzoate and amyl4-(dimethylamino)-benzoate;

[0082] esters of cinnamic acid, preferably 2-ethylhexyl4-methoxycinnamate, propyl 4-methoxycinnamate, isoamyl4-methoxycinnamate, 2-ethylhexyl 2-cyano-3,3-phenyl-cinnamate(octocrylene);

[0083] esters of salicylic acid, preferably 2-ethylhexyl salicylate,4-isopropylbenzyl salicylate, homomenthyl salicylate;

[0084] derivatives of benzophenone, preferably2-hydroxy-4-methoxybenzophenone,2-hydroxy-4-methoxy-4′-methyl-benzophenone,2,2′-dihydroxy-4-methoxybenzophenone;

[0085] esters of benzalmalonic acid, preferably di-2-ethyl-hexyl4-methoxybenzalmalonate;

[0086] triazine derivatives, such as, for example, 2,4,6-trianilino(p-carbo-2′-ethyl-1′-hexyloxy)-1,3,5-triazine and octyltriazone, asdescribed in EP 0818450 A1 or dioctylbutamidotriazone (Uvasorb® HEB);

[0087] propane-1,3-diones, such as, for example,1-(4-tert-butylphenyl)-3-(4′-methoxyphenyl)propane-1,3-dione;

[0088] ketotricyclo(5.2.1.0)decane derivatives, as described in EP0694521 B1.

[0089] Suitable water-soluble substances are:

[0090] 2-phenylbenzimidazole-5-sulfonic acid and the alkali metal,alkaline earth metal, ammonium, alkylammonium, alkanolammonium andglucammonium salts thereof;

[0091] sulfonic acid derivatives of benzophenones, preferably2-hydroxy-4-methoxybenzophenone-5-sulfonic acid and its salts;

[0092] sulfonic acid derivatives of 3-benzylidenecamphor, such as, forexample, 4-(2-oxo-3-bornylidenemethyl)-benzenesulfonic acid and2-methyl-5-(2-oxo-3-bornyl-idene)sulfonic acid and salts thereof.

[0093] Suitable typical UV-A filters are, in particular, derivatives ofbenzoylmethane, such as, for example,1-(4′-tert-butylphenyl)-3-(4′-methoxyphenyl)propane-1,3-dione,4-tert-butyl-4′-methoxydibenzoylmethane (Parsol 1789),1-phenyl-3-(4′-isopropylphenyl)propane-1,3-dione, and enamine compounds,as described in DE 19712033 A1 (BASF). The UV-A and UV-B filters can ofcourse also be used in mixtures. As well as said soluble substances,insoluble light protection pigments, namely finely dispersed metaloxides or salts, are also suitable for this purpose. Examples ofsuitable metal oxides are, in particular, zinc oxide and titaniumdioxide and also oxides of iron, zirconium, silicon, manganese, aluminumand cerium, and mixtures thereof. Salts which may be used are silicates(talc), barium sulfate or zinc stearate. The oxides and salts are usedin the form of the pigments for skincare and skin-protective emulsionsand decorative cosmetics. The particles here should have an averagediameter of less than 100 nm, preferably between 5 and 50 nm and inparticular between 15 and 30 nm. They can have a spherical shape, but itis also possible to use particles which have an ellipsoidal shape or ashape deviating in some other way from the spherical form. The pigmentscan also be surface-treated, i.e. hydrophilicized or hydrophobicized.Typical examples are coated titanium dioxides, such as, for example,titanium dioxide T 805 (Degussa) or Eusolex® T2000 (Merck). Suitablehydrophobic coating agents are here primarily silicones and,specifically in this case, trialkoxyoctylsilanes or simethicones. Insunscreens, preference is given to using so-called micro- ornanopigments. Preference is given to using micronized zinc oxide.Further suitable UV light protection filters are given in the review byP. Finkel in SÖFW-Journal 122, 543 (1996) and Parfümerie und Kosmetik 3(1999), page 11ff.

[0094] As well as the two abovementioned groups of primary lightprotection substances, it is also possible to use secondary lightprotection agents of the antioxidant type; these interrupt thephotochemical reaction chain which is triggered when WV radiationpenetrates the skin. Typical examples thereof are amino acids (e.g.glycine, histidine, tyrosine, tryptophan) and derivatives thereof,imidazoles (e.g. urocanic acid) and derivatives thereof, peptides, suchas D,L-carnosine, D-carnosine, L-carnosine and derivatives thereof (e.g.anserine), carotenoids, carotenes (e.g. α-carotene, 0-carotene,lycopene) and derivatives thereof, chlorogenic acid and derivativesthereof, lipoic acid and derivatives thereof (e.g. dihydrolipoic acid),aurothioglucose, propylthiouracil and other thiols (e.g. thioredoxin,glutathione, cysteine, cystine, cystamine and the glycosyl, N-acetyl,methyl, ethyl, propyl, amyl, butyl and lauryl, palmitoyl, oleyl,γ-linoleyl, cholesteryl and glyceryl esters thereof) and salts thereof,dilauryl thiodipropionate, distearyl thiodipropionate, thiodipropionicacid and derivatives thereof (esters, ethers, peptides, lipids,nucleotides, nucleosides and salts), and sulfoximine compounds (e.g.buthionine sulfoximines, homocysteine sulfoximine, buthionine sulfones,penta-, hexa-, heptathionine sulfoximine) in very low tolerated doses(e.g. pmol to μmol/kg), and also (metal) chelating agents (e.g.α-hydroxy fatty acids, palmitic acid, phytic acid, lactoferrin),αhydroxy acids (e.g. citric acid, lactic acid, malic acid), humic acid,bile acid, bile extracts, bilirubin, biliverdin, EDTA, EGTA andderivatives thereof, unsaturated fatty acids and derivatives thereof(e.g. γ-linolenic acid, linoleic acid, oleic acid), folic acid andderivatives thereof, ubiquinone and ubiquinol and derivatives thereof,vitamin C and derivatives (e.g. ascorbyl palmitate, Mg ascorbylphosphate, ascorbyl acetate), tocopherols and derivatives (e.g. vitaminE acetate), vitamin A and derivatives (vitamin A palmitate), andconiferyl benzoate of gum benzoin, rutic acid and derivatives thereof,α-glycosylrutin, ferulic acid, furfurylideneglucitol, carnosine,butylhydroxytoluene, butylhydroxyanisole, nordihydroguaiacic acid,nordihydroguaiaretic acid, trihydroxybutyrophenone, uric acid andderivatives thereof, mannose and derivatives thereof, superoxidedismutase, zinc and derivatives thereof (e.g. ZnO, ZnSO₄) selenium andderivatives thereof (e.g. selenomethionine), stilbenes and derivativesthereof (e.g. stilbene oxide, trans-stilbene oxide) and the derivatives(salts, esters, ethers, sugars, nucleotides, nucleosides, peptides andlipids) of said active ingredients which are suitable according to theinvention.

[0095] Biogenic Active Ingredients The term “biogenic activeingredients” means, for example, tocopherol, tocopherol acetate,tocopherol palmitate, ascorbic acid, (deoxy)ribonucleic acid, andfragments thereof, retinol, bisabolol, allantoin, phytantriol,panthenol, AHA acids, amino acids, ceramides, pseudoceramides, essentialoils, plant extracts and vitamin complexes.

[0096] Deodorants and Antimicrobial Agents

[0097] Cosmetic deodorants counteract, mask or remove body odors. Bodyodors arise as a result of the effect of skin bacteria on apocrineperspiration, with the formation of degradation products which have anunpleasant odor. Accordingly, deodorants comprise active ingredientswhich act as antimicrobial agents, enzyme inhibitors, odor absorbers orodor masking agents. Suitable antimicrobial agents are, in principle,all substances effective against Gram-positive bacteria, such as, forexample, 4-hydroxybenzoic acid and its salts and esters,N-(4-chlorophenyl)-N′-(3,4-dichlorophenyl)urea,2,4,4′-trichloro-2′-hydroxydiphenyl ether (triclosan),4-chloro-3,5-dimethylphenol, 2,2′-methylenebis(6-bromo-4-chlorophenol),3-methyl-4-(1-methylethyl)phenol, 2-benzyl-4-chlorophenol,3-(4-chlorophenoxy)-1,2-propanediol, 3-iodo-2-propynyl butylcarbamate,chlorhexidine, 3,4,4′-trichlorocarbanilide (TTC), antibacterialfragrances, thymol, thyme oil, eugenol, oil of cloves, menthol, mintoil, farnesol, phenoxyethanol, glycerol monocaprate, glycerolmonocaprylate, glycerol monolaurate (GML), diglycerol monocaprate (DMC),salicylic acid N-alkylamides, such as, for example, n-octylsalicylamideor n-decylsalicylamide.

[0098] Suitable enzyme inhibitors are, for example, esterase inhibitors.These are preferably trialkyl citrates, such as trimethyl citrate,tripropyl citrate, triisopropyl citrate, tributyl citrate and, inparticular, triethyl citrate (Hydagen® CAT, Henkel KGaA,Dusseldorf/FRG). The substances inhibit enzyme activity, therebyreducing the formation of odor. Other substances which are suitableesterase inhibitors are sterol sulfates or phosphates, such as, forexample, lanosterol, cholesterol, campesterol, stigmasterol andsitosterol sulfate or phosphate, dicarboxylic acids and esters thereof,such as, for example, glutaric acid, monoethyl glutarate, diethylglutarate, adipic acid, monoethyl adipate, diethyl adipate, malonic acidand diethyl malonate, hydroxycarboxylic acids and esters thereof, suchas, for example, citric acid, malic acid, tartaric acid or diethyltartrate, and zinc glycinate.

[0099] Suitable odor absorbers are substances which are able to absorband largely retain odor-forming compounds. They lower the partialpressure of the individual components, thus also reducing their rate ofdiffusion. It is important that in this process perfumes must remainunimpaired. Odor absorbers are not effective against bacteria. Theycomprise, for example, as main constituent, a complex zinc salt ofricinoleic acid or specific, largely odor-neutral fragrances which areknown to the person skilled in the art as “fixatives”, such as, forexample, extracts of labdanum or styrax or certain abietic acidderivatives. The odor masking agents are fragrances or perfume oils,which, in addition to their function as odor masking agents, give thedeodorants their respective fragrance note. Perfume oils which may bementioned are, for example, mixtures of natural and syntheticfragrances. Natural fragrances are extracts from flowers, stems andleaves, fruits, fruit peels, roots, woods, herbs and grasses, needlesand branches, and resins and balsams. Also suitable are animal rawmaterials, such as, for example, civet and castoreum. Typical syntheticfragrance compounds are products of the ester, ether, aldehyde, ketone,alcohol and hydrocarbon type. Fragrance compounds of the ester type are,for example, benzyl acetate, p-tert-butylcyclohexyl acetate, linalylacetate, phenylethyl acetate, linalyl benzoate, benzyl formate, allylcyclohexylpropionate, styrallyl propionate and benzyl salicylate. Theethers include, for example, benzyl ethyl ether, and the aldehydesinclude, for example, the linear alkanals having 8 to 18 carbon atoms,citral, citronellal, citronellyloxyacetaldehyde, cyclamen aldehyde,hydroxycitronellal, lilial and bourgeonal, the ketones include, forexample, the ionones and methyl cedryl ketone, the alcohols includeanethole, citronellol, eugenol, isoeugenol, geraniol, linaool,phenylethyl alcohol and terpineol, and the hydrocarbons include mainlythe terpenes and balsams. Preference is, however, given to usingmixtures of different fragrances which together produce a pleasingfragrance note. Essential oils of relatively low volatility, which aremostly used as aroma components, are also suitable as perfume oils, e.g.sage oil, camomile oil, oil of cloves, melissa oil, mint oil, cinnamonleaf oil, linden flower oil, juniperberry oil, vetiver oil, olibanumoil, galbanum oil, labdanum oil and lavandin oil. Preference is given tousing bergamot oil, dihydromyrcenol, lilial, lyral, citronellol,phenylethyl alcohol, α-hexylcinnamaldehyde, geraniol, benzylacetone,cyclamen aldehyde, linalool, boisambrene forte, ambroxan, indole,hedione, sandelice, lemon oil, mandarin oil, orange oil, allyl amylglycolate, cyclovertal, lavandin oil, clary sage oil, β-damascone,geranium oil bourbon, cyclohexyl salicylate, Vertofix coeur,iso-E-super, Fixolide NP, evernyl, iraldein gamma, phenylacetic acid,geranyl acetate, benzyl acetate, rose oxide, romilat, irotyl andfloramat alone or in mixtures.

[0100] Antiperspirants reduce the formation of perspiration byinfluencing the activity of the eccrine sweat glands, thus counteractingunderarm wetness and body odor. Aqueous or anhydrous formulations ofantiperspirants typically comprise the following ingredients:

[0101] astringent active ingredients,

[0102] oil components,

[0103] nonionic emulsifiers,

[0104] coemulsifiers,

[0105] bodying agents,

[0106] auxiliaries, such as, for example, thickeners or complexingagents and/or

[0107] nonaqueous solvents, such as, for example, ethanol, propyleneglycol and/or glycerol.

[0108] Suitable astringent antiperspirant active ingredients areprimarily salts of aluminum, zirconium or of zinc. Such suitableantihydrotic active ingredients are, for example, aluminum chloride,aluminum chlorohydrate, aluminum dichlorohydrate, aluminumsesquichlorohydrate and complex compounds thereof, e.g. with1,2-propylene glycol, aluminum hydroxyallantoinate, aluminum chloridetartrate, aluminum zirconium trichlorohydrate, aluminum zirconiumtetrachlorohydrate, aluminum zirconium pentachlorohydrate and complexcompounds thereof, e.g. with amino acids, such as glycine. In addition,customary oil-soluble and water-soluble auxiliaries may be present inantiperspirants in relatively small amounts. Such oil-solubleauxiliaries may, for example, be:

[0109] anti-inflammatory, skin-protective or perfumed essential oils,

[0110] synthetic skin-protective active ingredients and/or

[0111] oil-soluble perfume oils.

[0112] Customary water-soluble additives are, for example,preservatives, water-soluble fragrances, pH regulators, e.g. buffermixtures, water-soluble thickeners, e.g. water-soluble natural orsynthetic polymers, such as, for example, xanthan gum,hydroxyethylcellulose, poly-vinylpyrrolidone or high molecular weightpolyethylene oxides.

[0113] Film Formers

[0114] Customary film formers are, for example, chitosan,microcrystalline chitosan, quaternized chitosan, polyvinylpyrrolidone,vinylpyrrolidone-vinyl acetate copolymers, polymers of the acrylic acidseries, quaternary cellulose derivatives, collagen, hyaluronic acid andsalts thereof, and similar compounds.

[0115] Antidandruff Active Ingredients

[0116] Suitable antidandruff active ingredients are piroctone olamine(1-hydroxy-4-methyl-6-(2,4,4-trimythylpentyl)-2-(1H))-pyridinonemonoethanolamine salt), Baypival® (climbazole), ketoconazole®(4-acetyl-1-{4-[2-(2,4-dichlorophenyl)r-2-(1H-imidazol-1-ylmethyl)-1,3-dioxyl-anc-4-ylmethoxyphenyl}piperazine,selenium disulfide, colloidal sulfur, sulfur polyethylene glycolsorbitan monooleate, sulfur ricinol polyethoxylate, sulfur tardistillate, salicylic acid (or in combination with hexachlorophene),undexylenic acid monoethanolamide-sulfosuccinate Na salt, Lamepon® UD(protein undecylenic acid condensate), zinc pyrithione, aluminumpyrithione and magnesium pyrithione/dipyrithione magnesium sulfate.

[0117] Swelling Agents

[0118] The swelling agents for aqueous phases may be montmorillonites,clay mineral substances, Pemulen, and alkyl-modified Carbopol grades(Goodrich). Other suitable polymers and swelling agents are given in thereview by R. Lochhead in Corm. Toil. 108, 95 (1993).

[0119] Insect Repellents

[0120] Suitable insect repellents are N,N-diethyl-m-toluamide,1,2-pentanediol or ethyl butylacetylaminopropionate.

[0121] Self-Tanning Agents and Depigmentation Agents

[0122] A suitable self-tanning agent is dihydroxyacetone. Suitabletyrosine inhibitors, which prevent the formation of melanin and are usedin depigmentation compositions, are, for example, arbutin, kojic acid,coumaric acid and ascorbic acid (vitamin C).

[0123] Hydrotropic Agents

[0124] To improve the flow behavior, it is furthermore possible to usehydrotropic agents, such as, for example, ethanol, isopropyl alcohol orpolyols. Polyols which are suitable here preferably have 2 to 15 carbonatoms and at least two hydroxyl groups. The polyols can also containfurther functional groups, in particular amino groups, or can bemodified with nitrogen. Typical examples are

[0125] glycerol;

[0126] alkylene glycols, such as, for example, ethylene glycol,diethylene glycol, propylene glycol, butylene glycol, hexylene glycol,and polyethylene glycols having an average molecular weight of from 100to 1 000 daltons;

[0127] technical-grade oligoglycerol mixtures having a degree ofself-condensation of from 1.5 to 10, such as, for example,technical-grade diglycerol mixtures having a diglycerol content of from40 to 50% by weight;

[0128] methylol compounds, such as, in particular, trimethylolethane,trimethylolpropane, trimethylolbutane, pentaerythritol anddipentaerythritol;

[0129] lower alkyl glucosides, in particular those having 1 to 8 carbonatoms in the alkyl radical, such as, for example, methyl and butylglucoside;

[0130] sugar alcohols having 5 to 12 carbon atoms, such as, for example,sorbitol or mannitol;

[0131] sugars having 5 to 12 carbon atoms, such as, for example, glucoseor sucrose;

[0132] aminosugars, such as, for example, glucamine;

[0133] dialcohol amines, such as diethanolamine or2-amino-1,3-propanediol.

[0134] Preservatives

[0135] Suitable preservatives are, for example, phenoxy-ethanol,formaldehyde solution, parabens, pentanediol or sorbic acid, and theother classes of substance listed in Annex 6, Part A and B of theCosmetics Directive.

[0136] Perfume Oils

[0137] Perfume oils which may be mentioned are mixtures of natural andsynthetic fragrances. Natural fragrances are extracts from flowers(lily, lavender, rose, jasmine, neroli, ylang-ylang), stems and leaves(geranium, patchouli, petitgrain), fruits (aniseed, coriander, cumin,juniper), fruit peels (bergamot, lemon, orange), roots (mace, angelica,celery, cardamom, costus, iris, calmus), woods (pine wood, sandalwood,guaiac wood, cedarwood, rosewood), herbs and grasses (tarragon, lemongrass, sage, thyme), needles and branches (spruce, fir, pine,dwarf-pine), resins and balsams (galbanum, elemi, benzoin, myrrh,olibanum, opoponax). Also suitable are animal raw materials, such as,for example, civet and castoreum. Typical synthetic fragrance compoundsare products of the ester, ether, aldehyde, ketone, alcohol andhydrocarbon type. Fragrance compounds of the ester type are, forexample, benzyl acetate, phenoxyethyl isobutyrate,p-tert-butylcyclohexyl acetate, linalyl acetate, dimethylbenzylcarbinylacetate, phenylethyl acetate, linalyl benzoate, benzyl formate,ethylmethylphenyl glycinate, allyl cyclohexylpropionate, styrallylpropionate and benzyl salicylate. The ethers include, for example,benzyl ethyl ether, the aldehydes include, for example, the linearalkanals having 8 to 18 carbon atoms, citral, citronellal,citronellyloxyacetaldehyde, cyclamen aldehyde, hydroxycitronellal,lilial and bourgeonal, and the ketones include, for example, theionones, α-isomethylionone and methyl cedryl ketone, the alcoholsinclude anethol, citronellol, eugenol, isoeugenol, geraniol, linalool,phenylethyl alcohol and terpineol, and the hydrocarbons includepredominantly the terpenes and balsams. Preference is, however, given tousing mixtures of different fragrances which together produce a pleasingfragrance note. Essential oils, of relatively low volatility, which aremostly used as aroma components, are also suitable as perfume oils, e.g.sage oil, camomile oil, oil of cloves, melissa oil, mint oil, cinnamonleaf oil, linden blossom oil, juniperberry oil, vetiver oil, olibanumoil, galbanum oil, labolanum oil and lavandin oil. Preference is givento using bergamot oil, dihydromyrcenol, lilial, lyral, citronellol,phenylethyl alcohol, α-hexylcinnamaldehyde, geraniol, benzylacetone,cyclamen aldehyde, linalool, boisambrene forte, ambroxan, indole,hedione, sandelice, lemon oil, mandarin oil, orange oil, allyl amylglycolate, cyclovertal, lavandin oil, clary sage oil, β-damascone,geranium oil bourbon, cyclohexyl salicylate, Vertofix coeur,iso-E-super, Fixolide NP, evernyl, iraldein gamma, phenylacetic acid,geranyl acetate, benzyl acetate, rose oxide, romilllat, irotyl andfloramat alone or in mixtures.

[0138] Dyes

[0139] Dyes which can be used are the substances which are approved andsuitable for cosmetic purposes, as are listed, for example, in thepublication “Kosmetische Färbemittel” [Cosmetic Colorants] from theFarbstoffkommission der Deutschen Forschungsgemeinschaft [DyesCommission of the German Research Council], Verlag Chemie, Weinheim,1984, pp. 81-106. These dyes are normally used in concentrations of from0.001 to 0.1% by weight, based on the total mixture.

Examples Example 1

[0140] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a 50:50 mixture of cetearyl oligoglucoside and cetearyl alcohol(Emulgade® PL 68/50, Cognis Deutschland GmbH, melting point 640° C.) wasmade into drops at a rate of 0.7 kg/h/perforation. Starting from amelting temperature of 800° C., a product temperature of 21° C. wasestablished. Cooling took place with cold air at 3° C. from a fallingheight of 11 m. Dust-free flowable granules were obtained; theseconsisted of uniform beads, >70% of which had a size of 0.6 mm. Aproduct compressed with 780 kg/m² could, after a storage period of 2 h,be divided again into individual beads without problems. The productshowed no temperature increase as a result of residual heat. Thedissolution rate in hexyl laurate of the beads obtained in this way wastested as follows in comparison with a commercial product in the form ofprills: in each case 900 g of hexyl laurate were heated to 60° C.; inthis oil were dissolved, with stirring, amounts of 100 g in each case ofthe beads according to the invention and, for comparison, thecommercially available flakes. The dissolution rates determined were 8min for the beads according to the invention and 21 min for theconventional flaked product.

Example 2

[0141] In a Droppo-Line unit from Rieter Automatik GmbH with 0.5 mmnozzles, a 50:50 mixture of cetearyl oligoglucoside and cetearyl alcohol(Emulgade® PL 68/50) was made into drops at a rate of 2.5kg/h/perforation. Starting from a melting temperature of 80° C., aproduct temperature of 55° C. was established. Cooling was carried outusing cold air at 10° C. from a falling height of 11 m. Dust-freeflowable granules were obtained; these consisted of uniform beads, >70%of which had a size of 0.95 mm. A product compressed with 780 kg/m²could, after a storage period of 2 h, be divided again into individualbeads without problems. The product did not exhibit any increase intemperature as a result of residual heat. The dissolution rates in hexyllaurate determined were 9 min for the beads according to the inventionand 21 min for the conventional flaked product.

Example 3

[0142] In a Droppo-Line unit from Rieter Automatik GmbH with 0.5 mmnozzles, a 50:50 mixture of cocoalkyl oligoglucoside and polyglycerolpoly-12-hydroxystearate (Emulgin® VL 75, Cognis Deutschland GmbH) wasmade into drops at a rate of 1.1 kg/h/perforation. Starting from atemperature of 95° C., a product temperature of 65° C. was established.Cooling took place using cold air at 3° C. from a falling height of 11m. Dust-free flowable granules were obtained which consisted of uniformbeads, >70% of which had a size of 0.95 mm. Example 4

[0143] In a Droppo-Line unit from Rieter Automatik GmbH with 0.5 mmnozzles, a cetearyl alcohol (Lanette® O, Cognis Deutschland GmbH,melting point 51° C.) was made into drops at a rate of 2.5kg/h/perforation. Starting from a melting temperature of 65° C., aproduct temperature of 39° C. was established. Cooling was carried outwith cold air at 10° C. from a falling height of 11 m. Dust-freeflowable granules were obtained; these consisted of uniform beads, >70%of which had a size of 1 mm. A product compressed with 780 kg/m² could,after a storage period of 2 h, be divided again into individual beadswithout problems. The product did not exhibit any increase intemperature as a result of residual heat. The dissolution rates in hexyllaurate determined were 6 min for the beads according to the inventionand 12 min for the conventional flaked product.

Example 5

[0144] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a glycerol monostearate (Cutina® GMS-V, Cognis DeutschlandGmbH, melting point 59° C.) was made into drops at a rate of 2.0kg/h/perforation. Starting from a melting temperature of 7° C., aproduct temperature of 38° C. was established. Cooling took place withcold air at 3° C. from a falling height of 11 m. Dust-free flowablegranules were obtained; these consisted of uniform beads, >70% of whichhad a size of 0.65 mm. The dissolution rates determined were 8 min forthe beads according to the invention and 19 min for the conventionalflaked product.

Example 6

[0145] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 62° C.) of (a) 100 parts of a50:50 mixture of cetearyl oligoglucoside and cetearyl alcohol (Emulgade®PL 68/50), (b) 5 parts of sodium cetyl/stearyl sulfate (Lanette® E,Cognis Deutschland GmbH) and (c) 40 parts of glycerol monostearate(Cutina® GMS-V) were made into drops at a rate of 1.5 kg/h/perforation.Starting from a melting temperature of 75° C., a product temperature of43° C. was established. Cooling took place with cold air at 10° C. froma falling height of 11 m. Dust-free flowable granules were obtained;these consisted of uniform beads, >70% of which had a size of 0.65 mm.The dissolution rates determined were 21 min for the beads according tothe invention and 41 min for the conventional flaked product.

Example 7

[0146] In a Droppo-Line unit from Rieter Automatik GmbH with 0.5 mmnozzles, a mixture (melting temperature 62° C.) of (a) 100 parts of a50:50 mixture of cetearyl oligoglucoside and cetearyl alcohol (Emulgade®PL 68/50) and 10 parts of wheat protein hydrolyzate powder (Gluadin® WP,Cognis Deutschland GmbH) was made into drops at a rate of 1.5kg/h/perforation. Starting from a melting temperature of 75° C., aproduct temperature of 46° C. was established. Cooling was carried outwith cold air at 10° C. from a falling height of 11 m. Dust-freeflowable granules were obtained; these consisted of uniform beads, >70%of which had a size of 0.95 mm. The dissolution rates determined were 10min for the beads according to the invention and 21 min for theconventional flaked product.

Example 8

[0147] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 52° C.) of (a) 80 parts ofCutina® CBS (mixture of bodying waxes, Cognis Deutschland GmbH) (b) 15parts of ceteareth-12 (Eumulgin® B 1, Cognis Deutschland GmbH) and (c)15 parts of ceteareth-20 (Eumulgin® B 2, Cognis Deutschland GmbH) wasmade into drops at a rate of 1.5 kg/h/perforation. Starting from amelting temperature of 65° C., a product temperature of 38° C. wasestablished. Cooling was carried out with cold air at 10° C. from afalling height of 11 m. Dust-free flowable granules were obtained; theseconsisted of uniform beads, >70% of which had a size of 0.6 mm. Thedissolution rates determined were 16 min for the beads according to theinvention and 29 min for the conventional flaked product.

Example 9

[0148] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 55° C.) of 80 parts of stearicacid mono/diglyceride (Cutina® MD, Cognis Deutschland GmbH), (b) 8 partsof ceteareth-12 (Eumulgin B 1) and (c) [lacuna] parts of ceteareth-20(Eumulgin® B 2) were made into drops at a rate of 1.5 kg/h/perforation.Starting from a melting temperature of 70° C., a product temperature of45° C. was established. Cooling took place with cold air at 10° C. froma falling height of 11 m. Dust-free flowable granules were obtained;these consisted of uniform beads, >70% of which had a size of 0.6 mm.The dissolution rates determined were 14 min for the beads according tothe invention and 26 min for the conventional flaked product.

Example 10

[0149] In a Droppo-Line unit from Rieter Automatik GmbH with 0.5 mmnozzles, a mixture (melting temperature 56° C.) of 30 parts of cetearylalcohol (Lanette® O), (b) 40 parts of glycerol monostearate (Cutina®GMS-V) and (c) 8 parts of ceteareth-20 (Eumulgin® B 2) was made intodrops at a rate of 1.8 kg/h/perforation. Starting from a meltingtemperature of 65° C., a product temperature of 39° C. was established.Cooling took place with cold air at 10° C. from a falling height of 11m. Dust-free flowable granules were obtained; these consisted of uniformbeads, >70% of which had a size of 1 mm. The dissolution ratesdetermined were 8 min for the beads according to the invention and 15min for the conventional flaked product.

Example 11

[0150] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 48° C.) of (a) 20 parts ofstearic/palmitic acid (Cutina® FS 45, Cognis Deutschland GmbH), (b) 40parts of Cutina® CBS (mixture of bodying waxes) and (c) 10 parts of4-methylbenzylidenecamphor (Eusolex® 6300, Merck) was made into drops ata rate of 1.1 kg/h/perforation. Starting from a melting temperature of60° C., a product temperature of 31° C. was established. Cooling wascarried out with cold air at 10° C. from a falling height of 11 m.Dust-free flowable granules were obtained; these consisted of uniformbeads, >70% of which had a size of 0.6 mm. The dissolution ratesdetermined were 18 min for the beads according to the invention and 37min for the conventional flaked product.

Example 12

[0151] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 48° C.) of (a) 40 parts ofcetearyl alcohol (Lanette® O) and (b) 10 parts of benzophenone-3(NeoHeliopan® BB, Haarmann & Reimer) was made into drops at a rate of1.5 kg/h/perforation. Starting from a melting temperature of 60° C., aproduct temperature of 34° C. was established. Cooling was carried outwith cold air at 10° C. from a falling height of 11 m. Dust-freeflowable granules were obtained; these consisted of uniform beads, >70%of which had a size of 0.6 mm. The dissolution rates determined were 9minutes for the beads according to the invention and 16 min for theconventional flaked product.

Example 13

[0152] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 56° C.) of (a) 40 parts ofglycerol monostearate (Cutina® GMS-V) and (b) [lacuna] parts ofbenzophenone-3 (NeoHeliopan® BB) was made into drops at a rate of 1.5kg/h/perforation. Starting from a melting temperature of 70° C., aproduct temperature of 41° C. was established. Cooling was carried outwith cold air at 10° C. from a falling height of 11 m. Dust-freeflowable granules were obtained; these consisted of uniform beads, >70%of which had a size of 0.6 mm. The dissolution rates determined were 10min for the beads according to the invention and 18 min for theconventionally flaked product.

Example 14

[0153] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 51° C.) of (a) 45 parts ofcetearyl alcohol (Lanette® O) and (b) 10 parts of carotene was made intodrops at a rate of 1.3 kg/h/perforation. Starting from a meltingtemperature of 67° C., a product temperature of 38° C. was established.Cooling was carried out with cold air at 10° C. from a falling height of11 m. Dust-free flowable granules were obtained; these consisted ofuniform beads, >70% of which had a size of 0.6 mm. The dissolution ratesdetermined were 5 min for the beads according to the invention and 11min for the conventionally flaked product.

Example 15

[0154] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 53° C.) of (a) 45 parts ofcetearyl alcohol (Lanette® O) and (b) 7 parts of sodium cocoalkylsulfate (Sulfopon® 1218, Cognis Deutschland GmbH, 65% by weight ofactive substance) was made into drops at a rate of 1.0 kg/h/perforation(for this purpose, the melt was dispersed using a homogenizer (Supraton)and passed to the spraying tower). Starting from a melting temperatureof 70° C., a product temperature of 41° C. was established. Cooling wascarried out with cold air at 10° C. from a falling height of 11 m.Dust-free flowable granules were obtained; these consisted of uniformbeads, >70% of which had a size of 0.6 mm. The dissolution ratesdetermined were 7 min for the beads according to the invention and 13min for the conventional flaked product.

Example 16

[0155] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 53° C.) of (a) 50 parts ofcetearyl alcohol (Lanette® O) and (b) 4 parts of potassium cetylphosphate (25% by weight of active substance) was made into drops at arate of 1.1 kg/h/perforation (for this purpose, the melt was dispersedby means of a homogenizer (Supraton) and passed to the spraying tower).Starting from a melting temperature of 70° C., a product temperature of42° C. was established. Cooling was carried out with cold air at 10° C.from a falling height of 11 m. Dust-free flowable granules wereobtained; these consisted of uniform beads, >70% of which had a size of0.6 mm. The dissolution rates determined were 8 min for the beadsaccording to the invention and 15 min for the conventional flakedproduct.

Example 17

[0156] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 80° C.) of (a) 70 parts of atechnical-grade cocoalkyl polyglucoside mixture consisting of 80% byweight of glucoside and 20% by weight of fatty alcohol), and 30 parts ofa paste consisting of 50% by weight of cocoalkyl polyglucoside and 50%by weight of water (Plantacare® APG 1200, Cognis Deutschland GmbH) wasmade into drops at a rate of 0.80 kg/h/perforation (for this purpose,the melt was dispersed using a homogenizer (Supraton) and passed to thespraying tower). The mixture was fed into the drop-formation spray headat a temperature of 95° C. Cooling in the spraying tower with a fallingheight of 11 m took place with cold air at 10° C. Dust-free flowablegranules were obtained; these consisted of uniform beads, >70% of whichhad a size of 0.6 mm. The dissolution rate of the resulting beads wastested as follows in comparison with a corresponding product in flakedform: in each case 100 g of the pearl or flaked product were heated,with stirring, at 50° C. in 1 liter of water, the beads requiring onlyhalf of the time to dissolve which was necessary for dissolution of theflaked product. Example 18

[0157] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture of (a) 70 parts of C_(12/18)-fatty alcohol+20EO and(b) 30 parts of a paste consisting of 50% by weight of cocoalkylpolyglucoside and 50% by weight of water (Plantacare® APG 1200) was madeinto drops at a rate of 0.90 kg/h/perforation (for this purpose, themelt was dispersed using a homogenizer (Supraton) and passed to thespraying tower). The mixture was fed into the drop-formation spray headat a temperature of 95° C. Cooling in the spraying tower with a fallingheight of 11 m took place with cold air at 10° C. Dust-free flowablegranules were obtained; these consisted of uniform beads, >70% of whichhad a size of 0.6 mm. A product compressed with 500 kg/m² could, after astorage period of 2 h, be divided again into individual beads withoutproblems. The product did not exhibit any increase in temperature as aresult of residual heat. The dissolution rate of the resulting beads wastested as follows in comparison with a corresponding product in flakedform: in each case 100 g of the bead or flaked product were heated, withstirring, at 30° C. in 1 liter of water, the beads only requiring halfof the time to dissolve which was necessary for dissolution of theflaked product.

Example 19

[0158] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, a mixture (melting temperature 80° C.) of (a) 50 parts of atechnical-grade cocoalkyl polyglucoside mixture consisting of 80% byweight of glucoside and 20% by weight of fatty alcohol), and 50 parts ofC_(12/18)-fatty alcohol+20EO decyl ether was made into drops at a rateof 0.80 kg/h/perforation (for this purpose, the melt was dispersed usinga homogenizer (Supraton) and passed to the spraying tower). The mixturewas fed into the drop-formation spraying head at a temperature of 90° C.Cooling in the spraying tower with a falling height of 11 m was carriedout with cold air at 10° C. Dust-free flowable granules were obtained;these consisted of uniform beads, >70% of which had a size of 0.6 mm.The dissolution rate of the resulting beads was tested as follows incomparison with a corresponding product in flaked form: in each case 100g of the bead or flaked product were heated, with stirring, at 50° C. in1 liter of water, the beads requiring only half of the time to dissolvewhich was necessary for dissolution of the flaked product. Example 20

[0159] In a Droppo-Line unit from Rieter Automatik GmbH with 0.3 mmnozzles, stearic acid+40EO methyl ester (melting temperature 51° C.) wasmade into drops at a rate of 0.7 kg/h/perforation. Starting from amelting temperature of 65° C., a product temperature of 24° C. wasestablished. Cooling took place with cold air at 5° C. from a fallingheight of 11 m. Dust-free flowable granules were obtained; theseconsisted of uniform beads, >70% of which had a size of 0.6 mm. Thedissolution rate of the resulting beads was tested as follows incomparison with a corresponding product in flaked form: in each case 100g of the bead or flaked product were heated, with stirring, at 50° C. in1 liter of water, the beads requiring only half of the time to dissolvewhich was necessary for the dissolution of the flaked product. Example21

[0160] In a Droppo-Line unit from Rieter Automatik GmbH with 0.5 mmnozzles, a mixture (melting temperature 45° C.) of (a) 50 parts ofcoconut fatty acid +10EO methyl ester and (b) 50 parts of polyethyleneglycol (molecular weight 4 000) was made into drops at a rate of 1.7kg/h/perforation. Starting from a melting temperature of 75° C., aproduct temperature of 34° C. was established. Cooling took place withcold air at 15° C. from a falling height of 11 m. The resulting dropswere then powdered in silica. Dust-free flowable granules were obtained;these consisted of uniform beads, >70% of which had a size of 1 mm. Thedissolution rate of the resulting beads was tested as follows incomparison with a corresponding product in flaked form: in each case 100g of the bead or flaked product were heated, with stirring, at 50° C. in1 liter of water, the beads requiring only half of the time to dissolvewhich was necessary for the dissolution of the flaked product.

1. A granular solid with a monodisperse particle size distribution,obtainable by liquefying a predominantly anhydrous preparation which issolid at room temperature and comprises at least one cosmetic feedmaterial, making a stream of the melt into droplets using a castingplate by vibration, and passing a cooling medium countercurrently to thedroplets, which causes them to solidify.
 2. A process for thepreparation of granular solids with a monodisperse particle sizedistribution in which a predominantly anhydrous preparation which issolid at room temperature and which comprises at least one cosmetic feedmaterial is liquefied, a stream of the melt is made into droplets usinga casting plate by vibration and a cooling medium is passedcountercurrently to the droplets, which causes them to solidify.
 3. Theprocess as claimed in claim 2, characterized in that cosmetic feedmaterials are used which are chosen from the group formed byemulsifiers, wax bodies and bodying agents.
 4. The process as claimed inclaim 2 and/or 3, characterized in that the emulsifiers used arenonionic surfactants chosen from the group formed by alkyl and/oralkenyl oligoglycosides, fatty acid N-alkyl-polyhydroxyalkylamides,fatty alcohol polyglycol ethers, mixed ethers, alkoxylated fatty acidalkyl esters and polyol poly-12-hydroxystearates.
 5. The process asclaimed in at least one of claims 2 to 4, characterized in that waxbodies are used which are chosen from the group formed by natural waxes,synthetic waxes, lecithins, phospholipids and pearlescent waxes.
 6. Theprocess as claimed in at least one of claims 2 to 5, characterized inthat the bodying agents used are fatty alcohols and/or partialglycerides.
 7. The process as claimed in at least one of claims 2 to 6,characterized in that preparations are used which comprise less than 25%by weight of water.
 8. The process as claimed in at least one of claims2 to 7, characterized in that the cosmetic feed materials are usedtogether with further additives which are chosen from the group formedby UV light protection filters, antioxidants and biogenic activeingredients.
 9. The process as claimed in at least one of claims 2 to 8,characterized in that the preparations oscillate at a frequency of from100 to 1 000 Hz.
 10. The use of granular solids as claimed in claim 1for the preparation of surface-active preparations.